Development of ultrahigh-performance liquid chromatography/mass spectrometry and ultrahigh-performance supercritical fluid chromatography/mass spectrometry assays to determine the concentration of Bitrex™ and sodium saccharin in homemade facemask fit testing solutions.

Julie M Herniman,G John Langley

doi:10.1002/rcm.8848

Abstract

RationaleFast and easily transferable chromatography/mass spectrometry assays were required to detect and quantify the amount of Bitrex™ and sodium saccharin in homemade facemask fit testing solutions.MethodsBitrex™ solutions were analysed using reversed‐phase ultrahigh‐performance liquid chromatography coupled with positive ion electrospray ionisation mass spectrometry (UHPLC/ESI‐MS). Separation was achieved using a mobile phase gradient with an Acquity BEH C18‐packed column. Sodium saccharin solutions were analysed using ultrahigh‐performance supercritical fluid chromatography coupled with negative ion electrospray ionisation (UHPSFC/ESI‐MS). Separation was achieved using isocratic elution with an Acquity UPC2 Torus Diol packed column and a methanol (25 mM ammonium acetate) co‐solvent.ResultsThe calibration curves obtained using the ratio of the active compound to an internal standard generated linear regression values (R2) >0.99. Samples analysed prior to and after an autoclave sterilisation process and bottling gave repeatable measurements within 10% of the expected concentration.ConclusionsThe two assays afford a fast robust and quantitative analytical method for the detection of the active components used to test the efficacy of the homemade facemask testing solutions.

Highlights

In extreme environments where airborne pollutants may be present e.g. toxic gases, fumes, vapours, and other harmful pollutants, it is essential that personal protective equipment is worn and fitted correctly
It has a similar retention time to BitrexTM and its positive ion electrospray ionisation efficiency closely matched that of BitrexTM
The generic gradient was optimised to 20% solvent B increasing to 100% solvent B in 1.5 minutes with a 1-minute isocratic pre-run (Figure 3)

Summary

INTRODUCTION

In extreme environments where airborne pollutants may be present e.g. toxic gases, fumes, vapours, and other harmful pollutants, it is essential that personal protective equipment is worn and fitted correctly. Reversed phase UHPLC/MS methods were successfully developed for both BitrexTM and sodium saccharin, an alternative chromatographic technique, ultrahigh-performance supercritical fluid chromatography - mass spectrometry (UHPSFC/MS), was investigated for both assays. This would maximise usage of available instrumentation at the University of Southampton, Chemistry Mass Spectrometry Laboratory. The BitrexTM SENSE solution was prepared at a concentration of 135 mg/mL and this was serially diluted using methanol containing an internal standard oxybutynin chloride. (x 20,000 dilution) The saccharin SENSE solution was prepared at a concentration of 8.3 mg/mL and was serially diluted using methanol containing an internal standard vanillic acid. The TEST solution concentration was 536 mg/mL and it was serially diluted using methanol containing the same internal standard to a concentration of 26.8 ug/mL (x 20,000 dilution)

Chromatography

RESULTS AND DISCUSSION

CONCLUSIONS